Fluoropolymer lined metallic vessel design

ABSTRACT

The invention provides an apparatus useful in fluorinating organic compounds, or more particularly to a reactor system suitable for the fluorination of organic compounds on a commercial scale. The apparatus is also useful in chemical reactions including heating or cooling.

CROSS REFERENCE TO RELATED APPLICATION

This application is a division of U.S. patent application Ser. No.10/408,153, filed Apr. 4, 2003, now U.S. Pat. No. 7,102,040, which isincorporated herein by reference.

BACKGROUND OF THE INVENTION

The present invention relates to an apparatus useful for fluorinatingorganic compounds, or more particularly to a reactor suitable for thefluorination of organic compounds on a commercial scale. The reactor mayalso be used for other chemical processing that require heating orcooling. The reactor finds particular use in the manufacture ofhydroflurocarbons (HFCs). The reactor of the invention includes a largevolume reactor vessel lined with a loose fluoropolymer liner that ishighly resistive to corrosion.

It is known in the art that hydrofluorocarbons (HFCs) are popularsubstitutes for chlorofluorocarbons (CFCs) and hydrochlorofluorocarbons(HCFCs) for use as refrigerants, heat transfer agents, blowing agentsand propellants because HFCs do not deplete the ozone layer of theatmosphere. HFCs are typically prepared by fluorinating a chlorinatedorganic compound with a fluorination agent such as hydrogen fluoride inthe presence of a fluorination catalyst. This reaction may be conductedin either the liquid or gas phase. Generally, the liquid phasefluorination process is preferred because the reaction is controlled atrelatively lower temperatures which results in less by-product formationdue to decomposition.

Liquid phase fluorination, however, uses and generates corrosivecompounds, such as hydrogen fluoride, hydrogen chloride, and Lewis acidcatalysts, which form superacids. These superacids tend to corrode thereactor vessel in which the reaction is conducted, even reactorscomprised of corrosion-resistant materials such as Inconel 600,NAR25-50MII, Hastelloy C, Hastelloy G-30, duplex stainless steel, andHastelloy C-22. Corrosion of the reactor compromises the structuralintegrity of the reactor and reduces its useful life. Therefore, a needexists to minimize reactor corrosion.

One method of reducing such corrosion is taught in Japanese Kokai PatentApplication Publication No. 233102(1995). In this publication, a methodis disclosed for the liquid phase fluorination of a chlorinated organiccompound in a reactor made or lined with a fluorine containing resin.The method involves gaseous feeds of hydrogen fluoride and chlorinatedorganic compound. Because the process is restricted to gaseous feedstreams, it is limited in the type of HFCs it can produce. Chlorinatedorganic compounds having two or more carbon atoms tend to decomposebefore reaching their gaseous state. Thus, as a practical matter, theprocess disclosed in this publication can only be used to producefluorinated methanes.

The aforementioned Japanese publication also states that when heattransfer through the reactor is necessary, which is usually the case inliquid phase fluorination, the fluorine containing resin liner should beapplied using a molding method. The only molding method identifiedtherein is rotary-baked molding.

Generally, reactors having a molded liner, such as a rotary-baked orsprayed-on liner, are not suitable for large-scale commercialproduction. Reactors having such liners must be baked in large kilns orovens, which are expensive and frequently unavailable. Indeed, fitting alarge reactor, for example, greater than about a 1,000 gallons, with abaked liner is impractical.

A molded liner not only imposes practical limitations on the reactor,but also introduces structural limitations. It has been found thatmolded liners tend to be permeable and, under high pressures and overtime, reactants tend to penetrate the liner and develop pressure betweenthe liner and the reactor wall. Therefore, while a rotary-baked,fluorine-resin liner may minimize reactor corrosion, its structurallimitations nevertheless limit the reactor's useful lifetime.

To overcome these problems which are inherent with rotary-baked or spraymolded liners, it is now popular in the art to use a loose liner to linethe inside of reactors. As the term implies, a loose lining is one whichis fabricated from a sheet of protective material in a desiredconfiguration and which is then installed into the intended equipment.Capped flanges on the ends of the vessel are typically used to pressurefix the ends of the lining to the ends of the vessel.

Regarding fluorination reactions in particular, reactors that are linedwith a loose lining fabricated from fluoropolymer materials have beenfound to be useful for combating the corrosive conditions present incertain small-scale liquid phase fluorination reactions. For example,U.S. Pat. No. 5,902,912 teaches using a 50 gallon (appx. 6.7 ft³)loosely lined reactor vessel for producing less than one million lbs/yrof fluorocarbons in pilot scale operations. However, it has beendetermined that conventional non-corroding, fluoropolymer-lined reactorssuffer from a variety of problems when utilized in large-volumeprocesses, e.g. at least about 1000 gallons (appx. 134 ft³). Suchproblems include body flange seal leaking, liner flexing stress andshrinking, as well as leakage of hydrogen fluoride through the liner.Therefore, a need exists for non-corrosive reactors that can be used forthe commercial scale production of fluorinated compounds. Moreparticularly, there is a need for a high integrity, fluoropolymer linedmetallic vessel having a heat input/output capability suitable tomanufacture HFCs, such as HFC-143a, HFC-32, HFC-245fa, HFC-227ea,HFC-236fa, HFC-365mfc, etc., and to conduct other highly corrosiveapplications on a commercial scale.

The present invention provides a non-corroding and highly reliableapparatus useful for liquid phase hydrofluorination of organiccompounds. Furthermore, the invention provides a reactor apparatus thatavoids the problem of liner flexing and shrinking during disassembly ofthe reactor, and thus extending the operational life of the liner.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a side-view of a single stage reactor apparatus having oneshell member.

FIG. 2 is a side-view of a multi-stage reactor apparatus having aplurality of shell members.

FIG. 3 is a side view of two adjacent flanges having an intermediategasket.

FIG. 4 is a top view of an open reactor apparatus having a weep-hole.

FIG. 5 is a side view schematic representation of a bolt through aspring-loaded washer.

FIG. 6 is a top cross-sectional view of the reactor apparatus showingthe sequential bolting of the flanges and the secondary fasteners forthe lining.

DESCRIPTION OF THE INVENTION

The invention provides a reactor apparatus comprising:

a) a vessel comprising (i) or (ii):

-   -   i.) a single shell member        -   said shell member having a circumferential wall with an            inner surface which defines an interior cavity within the            inner surface; said shell member having a top shell member            opening at a top of the circumferential wall and a bottom            shell member opening at a bottom of the circumferential            wall, a first flange integrally formed with the shell member            around the circumferential wall at the top shell member            opening, which first flange extends outwardly            perpendicularly from the circumferential wall; a second            flange integrally formed with the shell member around the            circumferential wall at the bottom shell member opening,            which second flange extends outwardly perpendicularly from            the circumferential wall;    -   ii) a plurality of sequentially attached shell members,        -   each shell member having a circumferential wall with an            inner surface which defines an interior cavity within the            inner surface; each shell member having a top shell member            opening at a top of the circumferential wall and a bottom            shell member opening at a bottom of the circumferential            wall, a first flange integrally formed with the shell member            around the circumferential wall at the top shell member            opening, which first flange extends outwardly            perpendicularly from the circumferential wall; a second            flange integrally formed with the shell member around the            circumferential wall at the bottom shell member opening,            which second flange extends outwardly perpendicularly from            the circumferential wall;    -   the shell members being sequentially attached by mating adjacent        shell member flanges with an array of bolt and washer        combinations extending around and through the adjacent shell        member flanges; an intermediate gasket being positioned between        mating adjacent shell member flanges, said intermediate gasket        being positioned between the circumferential wall to the        circular array of bolt and washer combinations;

said vessel having a top opening at a top end thereof which is anuppermost top shell member opening, and a bottom opening at a bottom endthereof which is a lowermost bottom shell member opening;

b) a loose fluoropolymer liner lining the entire inner surface of eachcircumferential wall;

c) a top cover on the entire top opening of the vessel and on anuppermost of the shell member flanges, which top cover has an innersurface positioned on a first gasket, the first gasket being positionedon the uppermost shell member flange and said first gasket beingseparated from the uppermost shell member flange by a first end of theliner; the top cover being attached to the uppermost shell member flangeby an circular array of bolt and washer combinations extending aroundand through both the top cover and the uppermost shell member flange,said circular array of bolt and washer combinations being positionedbetween the circumferential wall and a terminal edge of the uppermostshell member flange; said first gasket being positioned between thecircumferential wall to the circular array of bolt and washercombinations;

d) a bottom cover on the entire bottom opening of the vessel and on alowermost of the shell member flanges, which bottom cover has an innersurface positioned on a second gasket, the second gasket beingpositioned on the lowermost shell member flange and said second gasketbeing separated from the lowermost shell member flange by a second endof the liner; the bottom cover being attached to the lowermost shellmember flange by a circular array of bolt and washer combinationsextending around and through both the bottom cover and the lowermostshell member flange, said circular array of bolt and washer combinationsbeing positioned between the circumferential wall and a terminal edge ofthe lowermost shell member flange; said second gasket being positionedbetween the circumferential wall to the circular array of bolt andwasher combinations;

e) a first end of the liner being attached to the uppermost shell memberflange by a circular array of screw fasteners extending around andthrough the uppermost shell member flange, which fasteners arepositioned between the circular array of bolt and washer combinationsand the terminal edge of the uppermost shell member flange; and a secondend of the liner being attached to the lowermost shell member flange bya circular array of screw fasteners extending around and through thelowermost shell member flange positioned between the circular array ofbolt and washer combinations and a terminal edge of the lowermost shellmember flange;

f) at least one inlet for supplying at least one fluid into saidinterior cavity; and

g) at least one outlet for discharging at least one fluid from saidinterior cavity.

The invention also provides a hydrofluorination process comprising:

I) providing a reactor apparatus as described above;

II) supplying a chlorinated organic material into said vessel throughsaid at least one inlet;

III) supplying hydrogen fluoride into said vessel through said at leastone inlet; and

IV) reacting the chlorinated organic material with said hydrogenfluoride to form a hydrofluorocarbon.

The invention further provides a process for forming hydrofluorocarbons,such as HFC-143a, HFC-32, HFC-245fa, HFC-227ea, HFC-236fa, HFC-365mfc,but not limited to these HFCs, by using the apparatus of the invention.

The invention still further provides a reaction process comprising:

I) providing a reactor apparatus comprising:

a) a vessel comprising (i) or (ii):

-   -   i.) a single shell member        -   said shell member having a circumferential wall with an            inner surface which defines an interior cavity within the            inner surface; said shell member having a top shell member            opening at a top of the circumferential wall and a bottom            shell member opening at a bottom of the circumferential            wall, a first flange integrally formed with the shell member            around the circumferential wall at the top shell member            opening, which first flange extends outwardly            perpendicularly from the circumferential wall; a second            flange integrally formed with the shell member around the            circumferential wall at the bottom shell member opening,            which second flange extends outwardly perpendicularly from            the circumferential wall;    -   ii) a plurality of sequentially attached shell members,        -   each shell member having a circumferential wall with an            inner surface which defines an interior cavity within the            inner surface; each shell member having a top shell member            opening at a top of the circumferential wall and a bottom            shell member opening at a bottom of the circumferential            wall, a first flange integrally formed with the shell member            around the circumferential wall at the top shell member            opening, which first flange extends outwardly            perpendicularly from the circumferential wall; a second            flange integrally formed with the shell member around the            circumferential wall at the bottom shell member opening,            which second flange extends outwardly perpendicularly from            the circumferential wall;

the shell members being sequentially attached by mating adjacent shellmember flanges with an array of bolt and washer combinations extendingaround and through the adjacent shell member flanges; an intermediategasket being positioned between mating adjacent shell member flanges,said intermediate gasket being positioned between the circumferentialwall to the circular array of bolt and washer combinations;

said vessel having a top opening at a top end thereof which is anuppermost top shell member opening, and a bottom opening at a bottom endthereof which is a lowermost bottom shell member opening;

b) a loose fluoropolymer liner lining the entire inner surface of eachcircumferential wall;

c) a top cover on the entire top opening of the vessel and on anuppermost of the shell member flanges, which top cover has an innersurface positioned on a first gasket, the first gasket being positionedon the uppermost shell member flange and said first gasket beingseparated from the uppermost shell member flange by a first end of theliner; the top cover being attached to the uppermost shell member flangeby an circular array of bolt and washer combinations extending aroundand through both the top cover and the uppermost shell member flange,said circular array of bolt and washer combinations being positionedbetween the circumferential wall and a terminal edge of the uppermostshell member flange; said first gasket being positioned between thecircumferential wall to the circular array of bolt and washercombinations;

d) a bottom cover on the entire bottom opening of the vessel and on alowermost of the shell member flanges, which bottom cover has an innersurface positioned on a second gasket, the second gasket beingpositioned on the lowermost shell member flange and said second gasketbeing separated from the lowermost shell member flange by a second endof the liner; the bottom cover being attached to the lowermost shellmember flange by a circular array of bolt and washer combinationsextending around and through both the bottom cover and the lowermostshell member flange, said circular array of bolt and washer combinationsbeing positioned between the circumferential wall and a terminal edge ofthe lowermost shell member flange; said second gasket being positionedbetween the circumferential wall to the circular array of bolt andwasher combinations;

e) a first end of the liner being attached to the uppermost shell memberflange by a circular array of screw fasteners extending around andthrough the uppermost shell member flange, which fasteners arepositioned between the circular array of bolt and washer combinationsand the terminal edge of the uppermost shell member flange; and a secondend of the liner being attached to the lowermost shell member flange bya circular array of screw fasteners extending around and through thelowermost shell member flange positioned between the circular array ofbolt and washer combinations and a terminal edge of the lowermost shellmember flange;

f) at least one inlet for supplying at least one fluid into saidinterior cavity; and

g) at least one outlet for discharging at least one fluid from saidinterior cavity.

II) supplying a first reagent into said vessel through said at least oneinlet;

III) supplying a second into said vessel through said at least oneinlet; and

IV) reacting the first reagent with the second reagent to form areaction product.

The reactor is suitable for conducting high integrity chemicalprocessing under high pressures and high temperature, and for heattransferring under high pressures. Such processes include either liquidor gaseous phase fluorination, but the reactor is especially suited forsustaining the extremely corrosive conditions of liquid fluorinationreactions.

As shown in FIG. 1, the reactor 10 comprises one circumferential,metallic shell member 20 that defines an interior cavity 38 (FIG. 4)into which reactants are supplied. Metallic shell can be made of anytypes of metal as long as it can provide mechanical strength.Corrosion-resistant metals or metal alloys, such as stainless steel,nickel containing alloys such as Inconel alloys, Monel alloys,Hastelloys, and combinations thereof. are preferred. It is alsopreferred that the shell members of the invention are equipped with acarbon steel wall jacket. The shell member preferably has an internaldiameter of from about 4.0 feet to about 6 feet. However, the diametermay be wider or narrower.

The shell member 20 has a top opening at a top end and a bottom openingat a bottom end, with each end being sealed by a top cover 12 and abottom cover 18, respectively. Each cover is either flat or curved inshape and functions to seal their respective openings. In the preferredembodiment of the invention, each of the top cover 12 and bottom cover18 are flat to minimize liner welds. Each cover preferably comprises asolid metallic plate of approximately ¼ inch (6.35 mm) in thicknessfabricated from the same metal as the shell member (e.g. a nickelalloy). The metallic plate is then plug welded to a carbon steel backupplate.

Extending through the top cover 12 and into the interior cavity 38 is aninlet 22 which supplies fluids or gases or both into the interiorcavity. Also extending through the top cover 12 and into the cavity 38is an outlet 24 which allows for discharging fluids or gases or bothfrom the cavity 38. As seen in the figure, the reactor apparatus maysimilarly include an inlet 22 and an outlet 24 extending through thebottom cover 14 and into the cavity 38. While reference is made hereinto inlets and outlets in general terms, it should be understood that theinlets and outlets are simply access points through which a gas or fluidmay be either supplied to or discharged from the inside of the reactorvessel. Each inlet or outlet may vary in diameter size and each is to beequipped with a nozzle. The reactor apparatus may also includeadditional inlets and/or outlets as desired to maintain the integrity ofthe reactor apparatus and as required by particular reaction processes.It is preferable that the reactor apparatus be equipped with one or more2 to 6 inch (5.08 to 15.24 cm) wide reactor feed inlets, a 2 to 6 inch(5.08 to 15.24 cm) purge inlet, and an 12 to 30 inch (30.48 to 76.2 cm)reaction vapor outlet. Each shell members may also be equipped with atleast one 1 to 3 inch (2.54 to 7.62 cm) steam inlet and at least one 1to 3 inch (2.54 to 7.62 cm) condensate outlet. Either the top cover 12or bottom cover 18 or both may further be equipped with meters thatmeasure the pressure and/or temperature conditions within the reactorapparatus. For example, a reactor apparatus may be equipped with aninlet/outlet through which is attached a pressure gauge, and anotherthrough which is attached a temperature gauge. The reactor apparatus mayalso be equipped with sampling mounts as desired.

Integrally formed with the shell 20 at its top end and adjacent to thetop cover 12 is a first flange 14. Similarly, a second flange 16 isformed with the shell 20 at its bottom end, the second flange 16 beingadjacent to the bottom cover 18. Positioned between the top cover 12 andthe first flange 14, as well as between the second flange 16 and thebottom cover 18, is a gasket 28 as can be seen in FIG. 3. Each of theflanges is preferably comprised of the same metal used to form the shellmembers and covers. Suitable gasket materials include fluoropolymermaterials, such as polytrifluoroethylene (e.g. TaskLine® gaskets) orpolychlorotrifluoroethylene, and is preferably a high compressibilityfluoroplastic tape, e.g. Gortex® tape. Utilizing such highcompressibility fluoroplastic tape compensates for any unevenness of theliner between the flange joints. In the preferred embodiment of theinvention, each flange is at least twice the gasketing width. Theseextra wide flanges add extra support to the liner and helps to preventshrinkage of the liner. The gasket should extend from a point betweenthe edge of cavity 38 up to the edge of the bolts holes which attach theflanges 14 and 16 to their respective covers 12 and 18.

In the preferred embodiment of the invention, the shell member 20 alongwith first flange 14 and second flange 16 is formed such that size ofthe reactor apparatus may be expanded by adding additional shell members20. This embodiment is shown in FIG. 2. As seen in the figure,additional shell members 20 may be added such that the second (bottom)flange 16 mates with the first (top) flange 14 of an adjacent shellmember. As shown in FIG. 3, two adjacent flanges are also separated by agasket 28. In the preferred embodiment of the invention, each flange isat least about twice the width of the gaskets. Each of these shellmembers are substantially identical to each other, including thesupports and fittings, and are the shell members are interchangeable.

While FIG. 2 illustrates an example of a reactor having three shellmembers 20 joined together to form a single reactor vessel, it should beunderstood that the reactor apparatus 10 may include more or fewer thanthree shell members 20. Preferably the overall size of the reactorapparatus 10 is such that the interior cavity 38 contains a volume ofabout 10 ft³ or more. In the preferred embodiment of the invention, eachof the shell members with its integrally formed flanges preferably has alength of from about 7 feet to about 8 feet. However, it should beunderstood that each shell member may be longer or shorter in length.

Lining all exposed interior surfaces of the reactor, including the innersurfaces of each of the top cover 12 and the bottom cover 18, is a loosefluoropolymer liner 30, shown in FIG. 4. As used herein, a “loosefluoropolymer liner” broadly refers to a liner which is fitted from afilm or sheet of a fluoropolymer material and which covers the innermetallic surfaces of the reactor. Specifically, the liner 30 insulatesall internal metal surfaces from corrosive reactants or reactionproducts present inside the reactor, but is not permanently molded tothe reactor. A loose liner differs from a molded liner in that a looseliner is not sprayed-on or rotary-baked from liquid form, but is apre-fabricated sheet material which is supported in the reactor. As isknown in the art, molded liners are coated onto the entire insidesurface of a reactor vessel and are generally useful in small scalemanufacturing applications. However, molded liners are very expensive tofabricate and are impractical for fitting large reactors. One mainproblem with molded liners is that they are known to break downstructurally when placed under high pressures and when used over a longperiod of time. On the other hand, a loose liner is capable ofwithstanding very high pressures and very high temperatures, and iseasily replaceable. Additionally, a loose liner is less porous thanmolded liners, has better overall strength and is not limited inthickness.

The loose liner 30 is positioned into the reactor vessel usingconventional application techniques, and is flared between two adjacentflanges 14 and 16 (or between top cover 12 and flange 14 and betweenflange 16 and bottom cover 18) such that the flanges fix the liner tothe vessel. As mentioned above, the flanges are at least about twice aswide as the gasket between the flanges. Flanges that are at least abouttwice as wide as the gasket width allow for self-regulating sealingpressure and reduces liner stress at the flange joints. This also avoidsover-compressing the liner 30 between the flanges, yet maximizes thereliability of the gasket sealability. It is also within the preferredembodiment of the invention that the liner 30 is secured in place withsecondary fasteners to hold the liner 30 in place during disassembly ofthe reactor apparatus 10.

As shown in FIG. 6, further supporting the liner in the vessel are aplurality of secondary fasteners 46, preferably fastening screws thatpenetrate through the liner and are fixed to the flanges. The liner isinitially fixed to the vessel at the flanges whereby a portion of theliner is flared onto a surface of one flange, wherein a second flange(or a cover) is then pressed onto the first flange, thus holding theliner between the two flanges. The dotted line shown in FIG. 6represents the boundary of the gasket 28, which preferably only extendsfrom the edge of interior cavity 38 to the edge of bolt holes 44. Asalso shown in the figure, the secondary fasteners 46 are then insertedthrough the liner and connected to at least one of the adjacent flangesto further support the liner against the flange.

These fasteners 46 function primarily to hold the liner in place duringdisassembly. This is an especially advantageous feature of the inventionbecause it avoids complications associated with liner shrinking. Morespecifically, it has been found that upon disassembly of a reactorapparatus having a loose fluoropolymer liner that has experienced someextended use, the liner has exhibited some shrinkage in size.Accordingly, once the liner is released from its fixed position betweenadjacent flanges, the liner no longer fits and cannot be replaced uponreassembly of the reactor apparatus. Therefore, a new liner must befitted to the vessel, which is very costly. It has been unexpectedlyfound that by further securing the liner 30 with such an array ofsecondary fasteners 46 that the liner may be held in place duringdisassembly of the reactor apparatus, preventing any recoil andshrinkage of the liner. The secondary fasteners 46 are preferablypositioned between the bolt holes 44 and the outermost edge of theflange. In order to confirm the tightness of the liner to the flangejoint and provide quality assurance to the final reactor installation, ahydrotest of the liner may be conducted.

In the preferred embodiment of the invention, the fluoropolymer linerpreferably comprises a polymer selected from the group consisting of,but not limited to, fluorinated ethylene propylene, poly(vinylidenefluoride), polytetrafluoroethylene, perfluoroalkoxy polymer, ethylenetetrafluoroethylene, ethylene hexafluoropropylene,tetrafluoroethylene-hexafluoropropylene, polychlorotrifluoroethylene,ethylene chlorotrifluoroethylene and combinations thereof. Of these,polytrifluoroethylene and perfluoroalkoxy copolymer are the mostpreferred fluoropolymers. In the preferred embodiment of the invention,the liner sheet has a thickness of about 0.5 mm to about 15 mm, morepreferably from about 3 mm to about 13 mm, and most preferably fromabout 5 to about 10 mm. However, it should be understood that suchthicknesses may vary as determined by individual uses and applicationsof the reactor apparatus.

As illustrated in FIG. 6, the flanges are bolted together through boltholes 44 using an circular array of bolt and washer combinationsextending around and through the flanges. Sequential bolt torqueingaround the flanges provides an evenly distributed bolting force on theflange sealing gaskets. The bolt seals are preferably continuouslymonitored by an on-stream ultrasonic bolt load monitoring system. Suchmonitoring provides instant and constant monitoring of the integrity ofthe flange seals, allowing for preventive measurements against theformation of leaks. In addition, in order to reduce costs, torsiontorque control may be used for practical tightening using inexpensiveair-driven impact wrenches.

Positioned between each bolt and each flange are spring-loaded washers40. This can be seen in FIG. 5. A spring loaded washer is a compactspring in the shape of a washer that has been pressed into a dishedshape and then hardened and tempered. One particularly preferred springloaded washer for use in assembling the reactor apparatus is aBelleville washer. A Belleville washer is a disk spring that appliespressure to the connection once you clamp down on it with the properamount of force. The advantage of this washer is that it appliesclamping pressure along a continuous arc pattern, instead ofconcentrating it at one point. Additionally, such Belleville washersprovide predictable bolting forces and maintains a positive sealingafter the reactor has experienced numerous repeated cycles of pressureand temperature changes.

In the preferred embodiment of the invention, the initial cold boltingforce on the spring washers is preferably from about 2,000 to about40,000 lbs. force/bolt, more preferably from about 10,000 to about33,000 lbs. force/bolt and most preferably from about 20,000 to about23,000 lbs. force/bolt.

In the preferred embodiment of the invention each shell member 20includes at least one weep hole 34 extending through the shell and tothe surface of the liner, and preferably a plurality of weep holes asseen in FIG. 4. These weep holes 34 are holes in the shell that allowreactants that permeate the fluoropolymer lining be vented out of thereactor. This prevents reactants from building up pressure between theliner and the shell wall and forming blisters in the liner. The weepholes are preferably from about 4.5 mm to about 10 mm in diameter, morepreferably from about 5.5 mm to about 8.5 mm, most preferably from about6.5 mm to about 8 mm. In the most preferred embodiment of the invention,each shell member 20 includes at least eight weep holes. As illustratedin FIG. 4, it is preferred that each shell member has four weep holes ateach of its top and bottom ends, with each weep hole being separatedfrom the next by 90° along the circumference of the shell member. Eachof the inlets and outlets are preferably also provided with a weep hole.Each weep hole 34 is preferably equipped with a ⅜ inch to 1½ inch (0.95to 3.8 cm) NPT coupling. Each coupling is preferably comprised of thesame metal used to form the shell member.

In the preferred embodiment of the invention, the weep holes areequipped with fluoroplastic inserts 32 that extend to the inner surfaceof the shell and reinforce the unsupported liner spots at the weep holes34. The fluoroplastic inserts 32 preferably comprise a fluoropolymermaterial selected from the group listed above. It is also preferred thatthe reactor apparatus further include an active vacuum system that isconnected to the weep hole system to prevent a vacuum collapse of theliner. This vacuum system prevents liner damage from vacuum collapsingin the event of improper operation of the reactor.

The reactor is also capable of being heated or cooled well enough tokeep the reaction temperature at a set, desired temperature, as well asat a desired pressure. In order to heat or cool the vessel, the reactorapparatus is equipped with jackets 26. Jackets 26, as shown in FIGS. 1and 2, preferably surround each shell member, and allow for controlledheating or cooling of the vessel. Jackets 26 are preferably spaced fromthe flanges to minimize excessive heating of the liner. In the preferredembodiment of the invention, the steam jacket is maintained at anoperating temperature of from about 40° C. to about and 375° C., morepreferably from about 65° C. to about 190° C. and most preferably fromabout 100° C. to about 155° C. The reactor is also preferably maintainedat an operating pressure of from about 15 psig to about 350 psig,preferably from about 30 psig to about 250 psig and more preferably fromabout 75 psig to about 200 psig. As also shown in FIG. 2, jackets 26 arepreferably supported by a support lug 36. While only a single supportlug 36 is shown in FIG. 2, it is preferred that each steam jacket 26 issupported by a separate support lug 36.

The reactor apparatus of the invention may further include additionalfeatures that are conventionally used for supporting a reactor apparatusor for further securing joints. For example, as shown in FIGS. 1 and 2,the reactor apparatus of the invention may include unit lifting and/orunit tailing trunions 42 at selected locations on the outer body of thereactor apparatus. The reactor apparatus may further include otherconventional features that are not shown in the drawings. For example,each of the covers and flanges preferably include lift lugs (at leasttwo with pads on each section of the apparatus), ground lugs (at leasttwo) and detector mounting clips that aid in the disassembly and/ormoving of the apparatus. Further, all carbon steel attachments to anickel alloy must include an attachment pad having a minimum thicknessof ¼ inch (6.35 mm).

It should be understood that the reactor apparatus may also includeadditional features not specifically mentioned herein as may beconventionally known by one skilled in the art, particularly featuresuseful for disassembling and moving the reactor apparatus.

The following non-limiting example serves to illustrate the invention.

EXAMPLE 1

A reactor apparatus is constructed as described above and having a 3,000gallon interior volume (11,353 Liters). The reactor is pre-charged withantimony pentachloride catalyst. A chlorinated organic and hydrogenfluoride are then introduced into the reactor. The operating reactionsof the reactor are set to 160 psig and 220° F. (104.4° C.), and steam isintroduced on the steam jacket to heat the reactor. The process yieldsat least 1,000 lb/hr (7.6 kg/min) of a hydrofluorocarbon, andaccumulates at least 2000 hours of operating time without leaks or linerdamage.

While the present invention has been particularly shown and describedwith reference to preferred embodiments, it will be readily appreciatedby those of ordinary skill in the art that various changes andmodifications may be made without departing from the spirit and scope ofthe invention. It is intended that the claims be interpreted to coverthe disclosed embodiment, those alternatives which have been discussedabove and all equivalents thereto.

1. A reactor apparatus comprising: (a) a vessel comprising (x) or (y):(x) a single shell member the shell member having a circumferential wallwith an inner surface which defines an interior cavity within the innersurface; the shell member having a top shell member opening at a top ofthe circumferential wall and a bottom shell member opening at a bottomof the circumferential wall, a first flange integrally formed with theshell member around the circumferential wall at the top shell memberopening, wherein the first flange extends outwardly perpendicularly fromthe circumferential wall; a second flange integrally formed with theshell member around the circumferential wall at the bottom shell memberopening, wherein the second flange extends outwardly perpendicularlyfrom the circumferential wall; (y) a plurality of sequentially attachedshell members, each shell member having a circumferential wall with aninner surface which defines an interior cavity within the inner surface;each shell member having a top shell member opening at a top of thecircumferential wall and a bottom shell member opening at a bottom ofthe circumferential wall, a first flange integrally formed with theshell member around the circumferential wall at the top shell memberopening, wherein the first flange extends outwardly perpendicularly fromthe circumferential wall; a second flange integrally formed with theshell member around the circumferential wall at the bottom shell memberopening, wherein the second flange extends outwardly perpendicularlyfrom the circumferential wall; the shell members being sequentiallyattached by mating adjacent shell member flanges with an array of boltand washer combinations extending around and through the adjacent shellmember flanges; an intermediate gasket being positioned between matingadjacent shell member flanges, each intermediate gasket being positionedbetween the circumferential wall to the circular array of bolt andwasher combinations; the vessel having a top opening at a top endthereof which is an uppermost top shell member opening, and a bottomopening at a bottom end thereof which is a lowermost bottom shell memberopening; (b) a loose fluoropolymer liner lining the entire inner surfaceof each circumferential wall; (c) a top cover on the entire top openingof the vessel and on an uppermost of the shell member flanges, whereinthe top cover has an inner surface positioned on a first gasket, thefirst gasket being positioned on the uppermost shell member flange andthe first gasket being separated from the uppermost shell member flangeby a first end of the liner; the top cover being attached to theuppermost shell member flange by a circular array of bolt and washercombinations extending around and through both the top cover and theuppermost shell member flange, the circular array of bolt and washercombinations being positioned between the circumferential wall and aterminal edge of the uppermost shell member flange; the first gasketbeing positioned between the circumferential wall to the circular arrayof bolt and washer combinations; (d) a bottom cover on the entire bottomopening of the vessel and on a lowermost of the shell member flanges,wherein the bottom cover has an inner surface positioned on a secondgasket, the second gasket being positioned on the lowermost shell memberflange and the second gasket being separated from the lowermost shellmember flange by a second end of the liner; the bottom cover beingattached to the lowermost shell member flange by a circular array ofbolt and washer combinations extending around and through both thebottom cover and the lowermost shell member flange, the circular arrayof bolt and washer combinations being positioned between thecircumferential wall and a terminal edge of the lowermost shell memberflange; the second gasket being positioned between the circumferentialwall to the circular array of bolt and washer combinations; (e) a firstend of the liner being attached to the uppermost shell member flange bya circular array of screw fasteners extending around and through theuppermost shell member flange, wherein the fasteners are positionedbetween the circular array of bolt and washer combinations and theterminal edge of the uppermost shell member flange; and a second end ofthe liner being attached to the lowermost shell member flange by acircular array of screw fasteners extending around and through thelowermost shell member flange positioned between the circular array ofbolt and washer combinations and a terminal edge of the lowermost shellmember flange; (f) at least one inlet for supplying at least one fluidinto the interior cavity; (g) at least one outlet for discharging atleast one fluid from the interior cavity; (h) wherein at least one shellfurther comprises at least one weep hole capable of transmitting gasesfrom between the interior cavity of the vessel and the liner to theoutside of the vessel, and (i) wherein the at least one weep holefurther comprises at least one fluoropolymer insert which extendsthrough the weep hole and into the vessel.
 2. A reactor apparatuscomprising: (a) a vessel comprising a single shell member; the shellmember having a circumferential wall with an inner surface which definesan interior cavity within the inner surface; the shell member having atop shell member opening at a top of the circumferential wall and abottom shell member opening at a bottom of the circumferential wall; afirst flange integrally formed with the shell member around thecircumferential wall at the top shell member opening, wherein the firstflange extends outwardly perpendicularly from the circumferential wall;a second flange integrally formed with the shell member around thecircumferential wall at the bottom shell member opening, wherein thesecond flange extends outwardly perpendicularly from the circumferentialwall; (b) a loose fluoropolymer liner lining the entire inner surface ofthe circumferential wall, wherein the liner is held in position suchthat recoil and shrinkage are prevented during disassembly of thereactor; (c) a top cover on the entire top opening of the vessel and onan uppermost of the shell member flanges, wherein the top cover has aninner surface positioned on a first gasket; the first gasket beingpositioned on the uppermost shell member flange and the first gasketbeing separated from the uppermost shell member flange by a first end ofthe liner; the top cover being attached to the uppermost shell memberflange by a circular array of bolt and washer combinations extendingaround and through both the top cover and the uppermost shell memberflange; the circular array of bolt and washer combinations beingpositioned between the circumferential wall and a terminal edge of theuppermost shell member flange; the first gasket being positioned betweenthe circumferential wall to the circular array of bolt and washercombinations; (d) a bottom cover on the entire bottom opening of thevessel and on a lowermost of the shell member flanges, wherein thebottom cover has an inner surface positioned on a second gasket; thesecond gasket being positioned on the lowermost shell member flange andthe second gasket being separated from the lowermost shell member flangeby a second end of the liner; the bottom cover being attached to thelowermost shell member flange by a circular array of bolt and washercombinations extending around and through both the bottom cover and thelowermost shell member flange; the circular array of bolt and washercombinations being positioned between the circumferential wall and aterminal edge of the lowermost shell member flange; the second gasketbeing positioned between the circumferential wall to the circular arrayof bolt and washer combinations; (e) a first end of the liner beingattached to the uppermost shell member flange by a circular array ofscrew fasteners extending around and through the uppermost shell memberflange, wherein the fasteners are positioned between the circular arrayof bolt and washer combinations and the terminal edge of the uppermostshell member flange; a second end of the liner being attached to thelowermost shell member flange by a circular array of screw fastenersextending around and through the lowermost shell member flangepositioned between the circular array of bolt and washer combinationsand a terminal edge of the lowermost shell member flange; (f) at leastone inlet for supplying at least one fluid into the interior cavity; (g)at least one outlet for discharging at least one fluid from the interiorcavity; (h) wherein the shell further comprises at least one weep holecapable of transmitting gases from between the interior cavity of thevessel and the liner to the outside of the vessel; and (i) wherein theat least one weep hole further comprises at least one fluoropolymerinsert which extends through the weep hole and into the vessel.
 3. Areactor apparatus comprising: (a) a vessel comprising a plurality ofsequentially attached shell members, each shell member having acircumferential wall with an inner surface which defines an interiorcavity within the inner surface; each shell member having a top shellmember opening at a top of the circumferential wall and a bottom shellmember opening at a bottom of the circumferential wall; a first flangeintegrally formed with the shell member around the circumferential wallat the top shell member opening, wherein the first flange extendsoutwardly perpendicularly from the circumferential wall; a second flangeintegrally formed with the shell member around the circumferential wallat the bottom shell member opening, wherein the second flange extendsoutwardly perpendicularly from the circumferential wall; the shellmembers being sequentially attached by mating adjacent shell memberflanges with an array of bolt and washer combinations extending aroundand through the adjacent shell member flanges; an intermediate gasketbeing positioned between mating adjacent shell member flanges; theintermediate gasket being positioned between the circumferential wall tothe circular array of bolt and washer combinations; the vessel having atop opening at a top end thereof which is an uppermost top shell memberopening, and a bottom opening at a bottom end thereof which is alowermost bottom shell member opening; (b) a loose fluoropolymer linerlining the entire inner surface of each circumferential wall, whereinthe liner is held in position such that recoil and shrinkage areprevented during disassembly of the reactor; (c) a top cover on theentire top opening of the vessel and on an uppermost of the shell memberflanges, wherein the top cover has an inner surface positioned on afirst gasket, the first gasket being positioned on the uppermost shellmember flange and the first gasket being separated from the uppermostshell member flange by a first end of the liner; the top cover beingattached to the uppermost shell member flange by a circular array ofbolt and washer combinations extending around and through both the topcover and the uppermost shell member flange, the circular array of boltand washer combinations being positioned between the circumferentialwall and a terminal edge of the uppermost shell member flange; the firstgasket being positioned between the circumferential wall to the circulararray of bolt and washer combinations; (d) a bottom cover on the entirebottom opening of the vessel and on a lowermost of the shell memberflanges, wherein the bottom cover has an inner surface positioned on asecond gasket, the second gasket being positioned on the lowermost shellmember flange and the second gasket being separated from the lowermostshell member flange by a second end of the liner; the bottom cover beingattached to the lowermost shell member flange by a circular array ofbolt and washer combinations extending around and through both thebottom cover and the lowermost shell member flange, the circular arrayof bolt and washer combinations being positioned between thecircumferential wall and a terminal edge of the lowermost shell memberflange; the second gasket being positioned between the circumferentialwall to the circular array of bolt and washer combinations; (e) a firstend of the liner being attached to the uppermost shell member flange bya circular array of screw fasteners extending around and through theuppermost shell member flange, wherein the fasteners are positionedbetween the circular array of bolt and washer combinations and theterminal edge of the uppermost shell member flange; and a second end ofthe liner being attached to the lowermost shell member flange by acircular array of screw fasteners extending around and through thelowermost shell member flange positioned between the circular array ofbolt and washer combinations and a terminal edge of the lowermost shellmember flange; (f) at least one inlet for supplying at least one fluidinto the interior cavity; (g) at least one outlet for discharging atleast one fluid from the interior cavity; (h) wherein the shell furthercomprises at least one weep hole capable of transmitting gases frombetween the interior cavity of the vessel and the liner to the outsideof the vessel; and (i) wherein the at least one weep hole furthercomprises at least one fluoropolymer insert which extends through theweep hole and into the vessel.
 4. The apparatus of claim 1, 2 or 3,wherein an inner surface of the top cover and an inner surface of thebottom cover comprise a fluoropolymer layer.
 5. The apparatus of claim1, 2 or 3, wherein the vessel contains at least 10 cubic feet of volume.6. The apparatus of claim 1, 2 or 3, wherein adjacent flanges, or aflange and the top cover, or a flange and the bottom cover are boltedtogether with spring-loaded washers.
 7. The apparatus of claim 1, 2 or3, wherein the fluoropolymer liner comprises a polymer selected from thegroup consisting of fluorinated ethylene propylene, poly(vinylidenefluoride), polytetrafluoroethylene, perfluoroalkoxy polymer, ethylenetetrafluoroethylene, ethylene hexafluoropropylene,tetrafluoroethylene-hexafluoropropylene, polychlorotrifluoroethylene,ethylene chlorotrifluoroethylene, polytrifluoroethylene and combinationsthereof.
 8. The apparatus of claim 1, 2 or 3, further comprising avacuum device connected to at least one weep hole.
 9. The apparatus ofclaim 1, 2 or 3, further comprising a heater for heating the vessel. 10.The apparatus of claim 9, wherein the heater comprises a steam jacketwhich surrounds the periphery of the at least one shell member.
 11. Theapparatus of claim 1, 2 or 3, wherein each shell member, each flange andeach cover comprises a material selected from the group consisting ofstainless steel, nickel containing alloys, and combinations thereof. 12.The apparatus of claim 1, 2 or 3, wherein at least one shell member isfurther equipped with an attachment pad having a minimum thickness ofabout 6.35 mm.
 13. The apparatus of claim 1, 2 or 3, wherein each shellmember has an internal diameter of about from about 4 feet to about 6feet.
 14. The apparatus of claim 1, 2 or 3, wherein each shell memberhas a length of from about 7 feet to about 8 feet measured from theouter surface of the first flange to the outer surface of the secondflange.